#------------------------------------------------------------------------------
#$Date: 2023-03-04 19:50:51 +0200 (Sat, 04 Mar 2023) $
#$Revision: 281352 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/83/1568315.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1568315
loop_
_publ_author_name
'Kobayashi, Yoshinao'
'Sunada, Yusuke'
_publ_section_title
;
 Germanium hydrides as an efficient hydrogen-storage material operated by
 an iron catalyst.
;
_journal_issue                   5
_journal_name_full               'Chemical science'
_journal_page_first              1065
_journal_page_last               1071
_journal_paper_doi               10.1039/d2sc06011f
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C40 H62 Fe N4'
_chemical_formula_sum            'C40 H62 Fe N4'
_chemical_formula_weight         654.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2022-09-01 deposited with the CCDC.	2022-12-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 107.412(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   20.0556(10)
_cell_length_b                   13.4841(5)
_cell_length_c                   16.4559(7)
_cell_measurement_reflns_used    11162
_cell_measurement_temperature    133
_cell_measurement_theta_max      31.25
_cell_measurement_theta_min      1.83
_cell_volume                     4246.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      133
_diffrn_detector_area_resol_mean 28.626
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19705
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.180
_diffrn_reflns_theta_min         1.848
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.024
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1424.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.31
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0681P)²+2.1911P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4607
_reflns_number_total             6256
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            d2sc06011f2.cif
_cod_data_source_block           Fe(iPrImMe)2(Mes)2
_cod_depositor_comments
'Adding full bibliography for 1568315--1568318.cif.'
_cod_database_code               1568315
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.500000 0.74838(2) 0.250000 0.01639(10) Uani 1 2 d S T P . .
N1 N 0.35038(7) 0.81364(10) 0.15767(9) 0.0204(3) Uani 1 1 d . . . . .
N2 N 0.34973(7) 0.68233(11) 0.23013(9) 0.0233(3) Uani 1 1 d . . . . .
C1 C 0.50051(8) 0.74776(12) 0.37524(10) 0.0202(3) Uani 1 1 d . . . . .
C2 C 0.52836(8) 0.66870(13) 0.43121(11) 0.0228(3) Uani 1 1 d . . . . .
C3 C 0.52786(9) 0.66855(15) 0.51590(11) 0.0296(4) Uani 1 1 d . . . . .
H3 H 0.546534 0.613139 0.550983 0.036 Uiso 1 1 calc R U . . .
C4 C 0.50098(10) 0.74673(15) 0.54968(11) 0.0335(4) Uani 1 1 d . . . . .
C5 C 0.47391(9) 0.82565(15) 0.49690(12) 0.0318(4) Uani 1 1 d . . . . .
H5 H 0.455752 0.880939 0.519162 0.038 Uiso 1 1 calc R U . . .
C6 C 0.47249(9) 0.82646(13) 0.41146(11) 0.0241(3) Uani 1 1 d . . . . .
C7 C 0.56053(9) 0.57981(13) 0.40190(12) 0.0291(4) Uani 1 1 d . . . . .
H7A H 0.553089 0.520783 0.432845 0.035 Uiso 1 1 calc R U . . .
H7B H 0.610774 0.590850 0.413125 0.035 Uiso 1 1 calc R U . . .
H7C H 0.538636 0.569988 0.340687 0.035 Uiso 1 1 calc R U . . .
C8 C 0.50101(14) 0.7464(2) 0.64124(14) 0.0523(6) Uani 1 1 d . . . . .
H8A H 0.452952 0.752860 0.643602 0.063 Uiso 1 1 calc R U . . .
H8B H 0.529022 0.802162 0.671430 0.063 Uiso 1 1 calc R U . . .
H8C H 0.521072 0.684017 0.668258 0.063 Uiso 1 1 calc R U . . .
C9 C 0.43925(10) 0.91496(14) 0.35905(12) 0.0314(4) Uani 1 1 d . . . . .
H9A H 0.447682 0.974271 0.395114 0.038 Uiso 1 1 calc R U . . .
H9B H 0.388822 0.903926 0.335571 0.038 Uiso 1 1 calc R U . . .
H9C H 0.459615 0.924254 0.312372 0.038 Uiso 1 1 calc R U . . .
C10 C 0.39423(8) 0.74846(11) 0.21087(10) 0.0187(3) Uani 1 1 d . . . . .
C11 C 0.28053(9) 0.78858(14) 0.14392(11) 0.0258(4) Uani 1 1 d . . . . .
C12 C 0.28016(9) 0.70633(15) 0.18934(12) 0.0292(4) Uani 1 1 d . . . . .
C13 C 0.37639(9) 0.90023(12) 0.12146(11) 0.0241(3) Uani 1 1 d . . . . .
H13 H 0.428477 0.898889 0.145189 0.029 Uiso 1 1 calc R U . . .
C14 C 0.35987(10) 0.89210(15) 0.02553(12) 0.0325(4) Uani 1 1 d . . . . .
H14A H 0.309367 0.898734 -0.001101 0.039 Uiso 1 1 calc R U . . .
H14B H 0.375398 0.827412 0.010912 0.039 Uiso 1 1 calc R U . . .
H14C H 0.384183 0.944888 0.004795 0.039 Uiso 1 1 calc R U . . .
C15 C 0.35278(11) 0.99871(13) 0.14840(14) 0.0366(5) Uani 1 1 d . . . . .
H15A H 0.357296 0.996743 0.209342 0.044 Uiso 1 1 calc R U . . .
H15B H 0.303859 1.010679 0.115924 0.044 Uiso 1 1 calc R U . . .
H15C H 0.381957 1.052217 0.137287 0.044 Uiso 1 1 calc R U . . .
C16 C 0.21951(9) 0.84290(16) 0.08683(14) 0.0370(5) Uani 1 1 d . . . . .
H16A H 0.176132 0.815266 0.093125 0.044 Uiso 1 1 calc R U . . .
H16B H 0.219565 0.835791 0.027579 0.044 Uiso 1 1 calc R U . . .
H16C H 0.222779 0.913306 0.102299 0.044 Uiso 1 1 calc R U . . .
C17 C 0.37507(9) 0.59838(13) 0.28828(11) 0.0271(4) Uani 1 1 d . . . . .
H17 H 0.427180 0.598825 0.302721 0.033 Uiso 1 1 calc R U . . .
C18 C 0.35073(12) 0.49771(15) 0.24723(14) 0.0400(5) Uani 1 1 d . . . . .
H18A H 0.357051 0.495442 0.190473 0.048 Uiso 1 1 calc R U . . .
H18B H 0.301209 0.488303 0.242262 0.048 Uiso 1 1 calc R U . . .
H18C H 0.378321 0.444894 0.282671 0.048 Uiso 1 1 calc R U . . .
C19 C 0.35835(10) 0.61102(15) 0.37151(12) 0.0334(4) Uani 1 1 d . . . . .
H19A H 0.307686 0.606953 0.361038 0.040 Uiso 1 1 calc R U . . .
H19B H 0.375191 0.675814 0.396204 0.040 Uiso 1 1 calc R U . . .
H19C H 0.381352 0.558474 0.411158 0.040 Uiso 1 1 calc R U . . .
C20 C 0.21833(10) 0.64942(19) 0.19711(14) 0.0464(6) Uani 1 1 d . . . . .
H20A H 0.216973 0.584261 0.170286 0.056 Uiso 1 1 calc R U . . .
H20B H 0.175431 0.685927 0.168692 0.056 Uiso 1 1 calc R U . . .
H20C H 0.222073 0.640792 0.257449 0.056 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Fe Fe 0.3463 0.8444
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C10 Fe1 C10 179.94(9) . 2_655 ?
C10 Fe1 C1 89.47(6) . 2_655 ?
C10 Fe1 C1 90.53(6) 2_655 2_655 ?
C10 Fe1 C1 90.53(6) . . ?
C10 Fe1 C1 89.47(6) 2_655 . ?
C1 Fe1 C1 179.53(9) 2_655 . ?
C10 N1 C11 111.90(14) . . ?
C10 N1 C13 122.17(13) . . ?
C11 N1 C13 125.92(14) . . ?
C10 N2 C12 111.51(14) . . ?
C10 N2 C17 122.09(13) . . ?
C12 N2 C17 126.39(14) . . ?
C2 C1 C6 114.95(15) . . ?
C2 C1 Fe1 122.65(12) . . ?
C6 C1 Fe1 122.40(12) . . ?
C3 C2 C1 122.22(16) . . ?
C3 C2 C7 116.72(16) . . ?
C1 C2 C7 121.06(15) . . ?
C4 C3 C2 121.54(17) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 117.74(17) . . ?
C3 C4 C8 121.29(19) . . ?
C5 C4 C8 120.97(19) . . ?
C4 C5 C6 121.70(17) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C1 121.83(17) . . ?
C5 C6 C9 117.03(16) . . ?
C1 C6 C9 121.14(15) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 N2 103.28(13) . . ?
N1 C10 Fe1 128.25(11) . . ?
N2 C10 Fe1 128.46(12) . . ?
C12 C11 N1 106.48(15) . . ?
C12 C11 C16 128.13(16) . . ?
N1 C11 C16 125.36(17) . . ?
C11 C12 N2 106.82(15) . . ?
C11 C12 C20 128.02(17) . . ?
N2 C12 C20 125.16(18) . . ?
N1 C13 C14 111.69(14) . . ?
N1 C13 C15 113.27(15) . . ?
C14 C13 C15 112.13(15) . . ?
N1 C13 H13 106.4 . . ?
C14 C13 H13 106.4 . . ?
C15 C13 H13 106.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C17 C19 112.01(15) . . ?
N2 C17 C18 113.15(15) . . ?
C19 C17 C18 111.81(15) . . ?
N2 C17 H17 106.4 . . ?
C19 C17 H17 106.4 . . ?
C18 C17 H17 106.4 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C12 C20 H20A 109.5 . . ?
C12 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C12 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C10 2.0240(15) . ?
Fe1 C10 2.0241(15) 2_655 ?
Fe1 C1 2.0578(16) 2_655 ?
Fe1 C1 2.0579(16) . ?
N1 C10 1.3607(19) . ?
N1 C11 1.392(2) . ?
N1 C13 1.475(2) . ?
N2 C10 1.364(2) . ?
N2 C12 1.393(2) . ?
N2 C17 1.471(2) . ?
C1 C2 1.410(2) . ?
C1 C6 1.413(2) . ?
C2 C3 1.397(2) . ?
C2 C7 1.507(2) . ?
C3 C4 1.375(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.378(3) . ?
C4 C8 1.507(3) . ?
C5 C6 1.398(2) . ?
C5 H5 0.9500 . ?
C6 C9 1.506(2) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 C12 1.339(3) . ?
C11 C16 1.493(2) . ?
C12 C20 1.496(3) . ?
C13 C14 1.517(3) . ?
C13 C15 1.520(2) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C19 1.514(3) . ?
C17 C18 1.530(3) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.2(2) . . . . ?
Fe1 C1 C2 C3 -179.38(13) . . . . ?
C6 C1 C2 C7 -179.58(15) . . . . ?
Fe1 C1 C2 C7 0.8(2) . . . . ?
C1 C2 C3 C4 -1.0(3) . . . . ?
C7 C2 C3 C4 178.78(16) . . . . ?
C2 C3 C4 C5 0.4(3) . . . . ?
C2 C3 C4 C8 -179.61(19) . . . . ?
C3 C4 C5 C6 1.0(3) . . . . ?
C8 C4 C5 C6 -178.99(19) . . . . ?
C4 C5 C6 C1 -1.8(3) . . . . ?
C4 C5 C6 C9 177.79(17) . . . . ?
C2 C1 C6 C5 1.2(2) . . . . ?
Fe1 C1 C6 C5 -179.22(13) . . . . ?
C2 C1 C6 C9 -178.46(16) . . . . ?
Fe1 C1 C6 C9 1.2(2) . . . . ?
C11 N1 C10 N2 -0.24(18) . . . . ?
C13 N1 C10 N2 178.99(14) . . . . ?
C11 N1 C10 Fe1 178.70(12) . . . . ?
C13 N1 C10 Fe1 -2.1(2) . . . . ?
C12 N2 C10 N1 0.23(18) . . . . ?
C17 N2 C10 N1 -178.89(14) . . . . ?
C12 N2 C10 Fe1 -178.71(12) . . . . ?
C17 N2 C10 Fe1 2.2(2) . . . . ?
C10 N1 C11 C12 0.2(2) . . . . ?
C13 N1 C11 C12 -179.03(16) . . . . ?
C10 N1 C11 C16 -178.01(17) . . . . ?
C13 N1 C11 C16 2.8(3) . . . . ?
N1 C11 C12 N2 0.0(2) . . . . ?
C16 C11 C12 N2 178.09(18) . . . . ?
N1 C11 C12 C20 179.5(2) . . . . ?
C16 C11 C12 C20 -2.4(4) . . . . ?
C10 N2 C12 C11 -0.1(2) . . . . ?
C17 N2 C12 C11 178.93(17) . . . . ?
C10 N2 C12 C20 -179.70(19) . . . . ?
C17 N2 C12 C20 -0.6(3) . . . . ?
C10 N1 C13 C14 114.31(17) . . . . ?
C11 N1 C13 C14 -66.6(2) . . . . ?
C10 N1 C13 C15 -117.93(17) . . . . ?
C11 N1 C13 C15 61.2(2) . . . . ?
C10 N2 C17 C19 110.49(18) . . . . ?
C12 N2 C17 C19 -68.5(2) . . . . ?
C10 N2 C17 C18 -122.02(18) . . . . ?
C12 N2 C17 C18 59.0(2) . . . . ?
